CN108249898A - A kind of preparation method of high-performance bullet proof composite plating - Google Patents
A kind of preparation method of high-performance bullet proof composite plating Download PDFInfo
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- CN108249898A CN108249898A CN201810061153.5A CN201810061153A CN108249898A CN 108249898 A CN108249898 A CN 108249898A CN 201810061153 A CN201810061153 A CN 201810061153A CN 108249898 A CN108249898 A CN 108249898A
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- proof composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000007747 plating Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000725 suspension Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 20
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 19
- 230000000694 effects Effects 0.000 claims abstract description 19
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 14
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 14
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 14
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 14
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 9
- 238000013019 agitation Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 159000000013 aluminium salts Chemical class 0.000 claims description 10
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 9
- 239000011154 composite armour Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 230000009189 diving Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000004702 methyl esters Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/83—Macromolecular compounds
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H5/00—Armour; Armour plates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of high-performance bullet proof composite plating, and aluminum soluble salt is added in deionized water, are then slowly added into ammonium hydroxide, stand 1 3h, add a dispersant in aluminium hydroxide suspension, 10 30min of ultrasonic reaction obtains suspended dispersion liquid；Graphene particles are added in absolute ethyl alcohol, then mechanical agitation seals 20 30min of ultrasonic reaction, obtain activated graphene suspension to dispersion effect is formed；Activated graphene suspension is slowly added into suspended dispersion liquid, rear gradient vacuum distillation 5 8h of reaction is stirred evenly, obtains viscous fluid；Viscous fluid is put into mold and is sintered 10 15h, 2 5h of ultrasonic reaction in polymethyl methacrylate solution, flash baking after taking-up are added in after natural cooling, 10 12h of gradient sintering obtains high-performance bullet proof composite plating after cooling.The present invention solves the problems, such as that existing overall performance is relatively low, has good bulletproof effect, greatly improves shellproof drag effect, is formed simultaneously more hard and soft collaboration protection.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of preparation method of high-performance bullet proof composite plating.
Background technology
The main polylith bulletproof ceramic block by shellproof backboard and on shellproof backboard of existing Ceramic Composite armour
It forms, although the cost performance of existing Ceramic Composite armour is very high, at least also there is such as this Ceramic Composite armour
Lower Railway Project：First, the overall weight of existing Ceramic Composite armour is generally higher；Second, prevent in existing Ceramic Composite
In diving board, the junction ballistic performance between bulletproof ceramic block is very weak；Third, the shellproof original of existing Ceramic Composite armour
Reason reaches shellproof purpose by increase bullet Penetration resistance, this shellproof principle limits existing Ceramic Composite armour
Overall performance it is relatively low.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of high-performance bullet proof composite plating, solves
The problem of existing overall performance is relatively low has good bulletproof effect, greatly improves shellproof drag effect, be formed simultaneously more
Hard and soft collaboration protection.
For realization more than technical purpose, the technical scheme is that：
A kind of preparation method of high-performance bullet proof composite plating, the preparation method is in accordance with the following steps：
Step 1, aluminum soluble salt is added in deionized water, is then slowly added into ammonium hydroxide, until precipitation no longer generates, it is quiet
1-3h is put, obtains aluminium hydroxide suspension；
Step 2, it adds a dispersant in aluminium hydroxide suspension, ultrasonic reaction 10-30min obtains suspended dispersion liquid；
Step 3, graphene particles are added in absolute ethyl alcohol, mechanical agitation is to dispersion effect is formed, and then sealing is ultrasonic
20-30min is reacted, obtains activated graphene suspension；
Step 4, activated graphene suspension is slowly added into suspended dispersion liquid, is uniformly mixing to obtain mixed liquor；
Step 5, mixed liquor is added in into reaction kettle and forms gradient vacuum distillation reaction 5-8h, obtain viscous fluid；
Step 6, viscous fluid is put into mold and is sintered 10-15h, polymethyl methacrylate solution is added in after natural cooling
Middle ultrasonic reaction 2-5h, flash baking after taking-up obtain the prefabricated armour of plated film；
Step 7, the prefabricated armour of plated film is added in into gradient sintering 10-12h in reaction kettle, it is compound obtains high-performance after cooling
Armour.
The aluminum soluble salt of the step 1 uses aluminium chloride, the mass concentration of the aluminum soluble salt in deionized water
For 10-30g/L.
It is 10-30mL/min that ammonia in the step 1, which adds in speed, and the dwell temperature is 60-70 DEG C.
For dispersant in the step 2 using polyvinylpyrrolidone, the addition of the dispersant is aluminium salt quality
20-40%, the frequency of the ultrasonic reaction is 2.5-7.5kHz, and temperature is 70-80 DEG C.
The grain size of graphene particles in the step 3 is not more than 100 μm, a concentration of 10-30g/ in absolute ethyl alcohol
L, the addition of the graphene particles is the 40-60% of aluminium salt, the churned mechanically speed be 2000-4000r/min, institute
It states sealing ultrasonic reaction to react using water bath sonicator, supersonic frequency 5.5-10.5kHz, temperature is 60-70 DEG C.
The addition speed of activated graphene suspension in the step 4 is 15-25mL/min, and the stirring of the stirring is fast
It spends for 2000-4000r/min.
Gradient vacuum distillation reaction in the step 5 uses microwave reaction, and Gradient program is as follows：
Sintering temperature in the step 6 is 1000-1200 DEG C, and the sintering processing is reacted using microwave heating, microwave
Power is 200-400W.
The solvent of polymethyl methacrylate solution uses acetone in the step 6, and the temperature of the ultrasonic reaction is 60-
70 DEG C, frequency 10-30kHz, the drying temperature is 70-90 DEG C.
Gradient sintering in the step 7 is sintered using Muffle furnace, and Gradient program is as follows：
| Temperature | Pressure | Time |
| 80-100℃ | 10-20MPa | 30-120min |
| 150-180℃ | 3-6MPa | 60-120min |
| 200-250℃ | 1-2MPa | Remaining time |
Step 1 forms precipitation using aluminum soluble salt under ammonium hydroxide effect, and forms aluminium hydroxide under static conditions and hang
Turbid.
Step 2, aluminium hydroxide suspension is added a dispersant to, and acts on dispersant to hydrogen-oxygen under ultrasonication
Change aluminium surface, form good dispersion.
Step 3, graphene particles are added in absolute ethyl alcohol, graphene is then blended in absolute ethyl alcohol by stirring
In, form suspension；Graphene ethanol is handled by the way of closed ultrasonic, graphene particles surface can be lived
Change, form the dispersion of activated graphene.
Step 4, activated graphene is added in into dispersion liquid, by churned mechanically mode by activated graphene and hydrogen-oxygen
Change aluminium to be thoroughly mixed, form mixed liquor.
Step 5 is slowly removed ethyl alcohol and deionized water by the way of gradient vacuum distillation, forms relatively stable glue
Magma, while viscous fluid not only with good dispersion effect, while itself has good due to containing polyvinylpyrrolidone
Toughness.
Step 6 adds in viscous fluid in mold, and the alumina material of graphene toughening, Ran Hou are formed in sintering process
Ultrasonic reaction in polymethyl methacrylate solution is filled up the gap in alumina material using polymethyl methacrylate,
Increase the connection effect of armour, not only with rigid connection, while also there is the elastic connection of high molecular material.
Step 7 can effectively promote the company between polymethyl methacrylate and aluminium oxide by way of gradient sintering
Effect is connect, greatly promotes the tensile strength of the two.
From the above, it can be seen that the present invention has advantages below：
1. the present invention solves the problems, such as that existing overall performance is relatively low, there is good bulletproof effect, greatly improve anti-
Elastic resistance acts on, and is formed simultaneously more hard and soft collaboration protection.
2. the present invention is configured to form floccule aluminum hydroxide precipitation using aluminum soluble salt with ammonium hydroxide, the gap between sediment
It is larger, suspended dispersion liquid can be formed.
3. the present invention is added in using the graphene of ultrasonic activation under the conditions of ethyl alcohol into aluminum hydroxide precipitation, can be formed compared with
For stable suspended system, and graphene can be inlayed to aluminum hydroxide precipitation, formed good gap and filled up effect.
4. the present invention can evaporate solvent successively by the way of gradient vacuum distillation, prevent evaporation of the solvent too fast, cause
Particle aggregation.
5. polyvinylpyrrolidone is sintered removal by the present invention by the way of sintering, and using polymethyl
Sour methyl esters is filled up agent as gap and can effectively be filled up gap, at the same can also be formed under the conditions of gradient sintering it is hard and soft simultaneously
The bullet proof composite plating of Ji.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of high-performance bullet proof composite plating, the preparation method is in accordance with the following steps：
Step 1, aluminum soluble salt is added in deionized water, is then slowly added into ammonium hydroxide, until precipitation no longer generates, it is quiet
1h is put, obtains aluminium hydroxide suspension；
Step 2, it adds a dispersant in aluminium hydroxide suspension, ultrasonic reaction 10min obtains suspended dispersion liquid；
Step 3, graphene particles are added in absolute ethyl alcohol, mechanical agitation is to dispersion effect is formed, and then sealing is ultrasonic
20min is reacted, obtains activated graphene suspension；
Step 4, activated graphene suspension is slowly added into suspended dispersion liquid, is uniformly mixing to obtain mixed liquor；
Step 5, mixed liquor is added in into reaction kettle and forms gradient vacuum distillation reaction 5h, obtain viscous fluid；
Step 6, viscous fluid is put into mold and is sintered 10h, added in polymethyl methacrylate solution after natural cooling
Ultrasonic reaction 2h, flash baking after taking-up obtain the prefabricated armour of plated film；
Step 7, the prefabricated armour of plated film is added in into gradient sintering 10h in reaction kettle, it is compound anti-that high-performance is obtained after cooling
Diving board.
The aluminum soluble salt of the step 1 uses aluminium chloride, the mass concentration of the aluminum soluble salt in deionized water
For 10g/L.
It is 10mL/min that ammonia in the step 1, which adds in speed, and the dwell temperature is 60 DEG C.
For dispersant in the step 2 using polyvinylpyrrolidone, the addition of the dispersant is aluminium salt quality
20%, the frequency of the ultrasonic reaction is 2.5kHz, and temperature is 70 DEG C.
The grain size of graphene particles in the step 3 is 100 μm, a concentration of 10g/L in absolute ethyl alcohol, the stone
The addition of black alkene particle is the 40% of aluminium salt, and the churned mechanically speed is 2000r/min, and the sealing ultrasonic reaction is adopted
It is reacted with water bath sonicator, supersonic frequency 5.5kHz, temperature is 60 DEG C.
The addition speed of activated graphene suspension in the step 4 be 15mL/min, the mixing speed of the stirring
For 2000r/min.
Gradient vacuum distillation reaction in the step 5 uses microwave reaction, and Gradient program is as follows：
Sintering temperature in the step 6 is 1000 DEG C, and the sintering processing is reacted using microwave heating, and microwave power is
200W。
The solvent of polymethyl methacrylate solution uses acetone in the step 6, and the temperature of the ultrasonic reaction is 60
DEG C, frequency 10kHz, the drying temperature is 70 DEG C.
Gradient sintering in the step 7 is sintered using Muffle furnace, and Gradient program is as follows：
| Temperature | Pressure | Time |
| 80℃ | 10MPa | 30min |
| 150℃ | 3MPa | 60min |
| 200℃ | 1MPa | Remaining time |
Embodiment 2
A kind of preparation method of high-performance bullet proof composite plating, the preparation method is in accordance with the following steps：
Step 1, aluminum soluble salt is added in deionized water, is then slowly added into ammonium hydroxide, until precipitation no longer generates, it is quiet
3h is put, obtains aluminium hydroxide suspension；
Step 2, it adds a dispersant in aluminium hydroxide suspension, ultrasonic reaction 30min obtains suspended dispersion liquid；
Step 3, graphene particles are added in absolute ethyl alcohol, mechanical agitation is to dispersion effect is formed, and then sealing is ultrasonic
30min is reacted, obtains activated graphene suspension；
Step 4, activated graphene suspension is slowly added into suspended dispersion liquid, is uniformly mixing to obtain mixed liquor；
Step 5, mixed liquor is added in into reaction kettle and forms gradient vacuum distillation reaction 8h, obtain viscous fluid；
Step 6, viscous fluid is put into mold and is sintered 15h, added in polymethyl methacrylate solution after natural cooling
Ultrasonic reaction 5h, flash baking after taking-up obtain the prefabricated armour of plated film；
Step 7, the prefabricated armour of plated film is added in into gradient sintering 12h in reaction kettle, it is compound anti-that high-performance is obtained after cooling
Diving board.
The aluminum soluble salt of the step 1 uses aluminium chloride, the mass concentration of the aluminum soluble salt in deionized water
For 30g/L.
It is 30mL/min that ammonia in the step 1, which adds in speed, and the dwell temperature is 70 DEG C.
For dispersant in the step 2 using polyvinylpyrrolidone, the addition of the dispersant is aluminium salt quality
40%, the frequency of the ultrasonic reaction is 7.5kHz, and temperature is 80 DEG C.
The grain size of graphene particles in the step 3 be 500nm, a concentration of 30g/L in absolute ethyl alcohol, the stone
The addition of black alkene particle is the 60% of aluminium salt, and the churned mechanically speed is 4000r/min, and the sealing ultrasonic reaction is adopted
It is reacted with water bath sonicator, supersonic frequency 10.5kHz, temperature is 70 DEG C.
The addition speed of activated graphene suspension in the step 4 be 25mL/min, the mixing speed of the stirring
For 4000r/min.
Gradient vacuum distillation reaction in the step 5 uses microwave reaction, and Gradient program is as follows：
Sintering temperature in the step 6 is 1200 DEG C, and the sintering processing is reacted using microwave heating, and microwave power is
400W。
The solvent of polymethyl methacrylate solution uses acetone in the step 6, and the temperature of the ultrasonic reaction is 70
DEG C, frequency 30kHz, the drying temperature is 90 DEG C.
Gradient sintering in the step 7 is sintered using Muffle furnace, and Gradient program is as follows：
| Temperature | Pressure | Time |
| 100℃ | 20MPa | 120min |
| 180℃ | 6MPa | 120min |
| 250℃ | 2MPa | Remaining time |
Embodiment 3
A kind of preparation method of high-performance bullet proof composite plating, the preparation method is in accordance with the following steps：
Step 1, aluminum soluble salt is added in deionized water, is then slowly added into ammonium hydroxide, until precipitation no longer generates, it is quiet
2h is put, obtains aluminium hydroxide suspension；
Step 2, it adds a dispersant in aluminium hydroxide suspension, ultrasonic reaction 20min obtains suspended dispersion liquid；
Step 3, graphene particles are added in absolute ethyl alcohol, mechanical agitation is to dispersion effect is formed, and then sealing is ultrasonic
25min is reacted, obtains activated graphene suspension；
Step 4, activated graphene suspension is slowly added into suspended dispersion liquid, is uniformly mixing to obtain mixed liquor；
Step 5, mixed liquor is added in into reaction kettle and forms gradient vacuum distillation reaction 7h, obtain viscous fluid；
Step 6, viscous fluid is put into mold and is sintered 13h, added in polymethyl methacrylate solution after natural cooling
Ultrasonic reaction 4h, flash baking after taking-up obtain the prefabricated armour of plated film；
Step 7, the prefabricated armour of plated film is added in into gradient sintering 11h in reaction kettle, it is compound anti-that high-performance is obtained after cooling
Diving board.
The aluminum soluble salt of the step 1 uses aluminium chloride, the mass concentration of the aluminum soluble salt in deionized water
For 20g/L.
It is 20mL/min that ammonia in the step 1, which adds in speed, and the dwell temperature is 65 DEG C.
For dispersant in the step 2 using polyvinylpyrrolidone, the addition of the dispersant is aluminium salt quality
30%, the frequency of the ultrasonic reaction is 5.5kHz, and temperature is 75 DEG C.
The grain size of graphene particles in the step 3 is 5 μm, a concentration of 20g/L in absolute ethyl alcohol, the graphite
The addition of alkene particle is the 50% of aluminium salt, and the churned mechanically speed is 3000r/min, and the sealing ultrasonic reaction uses
Water bath sonicator reacts, supersonic frequency 7.5kHz, and temperature is 65 DEG C.
The addition speed of activated graphene suspension in the step 4 be 20mL/min, the mixing speed of the stirring
For 3000r/min.
Gradient vacuum distillation reaction in the step 5 uses microwave reaction, and Gradient program is as follows：
Sintering temperature in the step 6 is 1100 DEG C, and the sintering processing is reacted using microwave heating, and microwave power is
300W。
The solvent of polymethyl methacrylate solution uses acetone in the step 6, and the temperature of the ultrasonic reaction is 65
DEG C, frequency 20kHz, the drying temperature is 80 DEG C.
Gradient sintering in the step 7 is sintered using Muffle furnace, and Gradient program is as follows：
| Temperature | Pressure | Time |
| 90℃ | 15MPa | 90min |
| 160℃ | 4MPa | 150min |
| 230℃ | 2MPa | Remaining time |
In conclusion the present invention has the following advantages：
1. the present invention solves the problems, such as that existing overall performance is relatively low, there is good bulletproof effect, greatly improve anti-
Elastic resistance acts on, and is formed simultaneously more hard and soft collaboration protection.
2. the present invention is configured to form floccule aluminum hydroxide precipitation using aluminum soluble salt with ammonium hydroxide, the gap between sediment
It is larger, suspended dispersion liquid can be formed.
3. the present invention is added in using the graphene of ultrasonic activation under the conditions of ethyl alcohol into aluminum hydroxide precipitation, can be formed compared with
For stable suspended system, and graphene can be inlayed to aluminum hydroxide precipitation, formed good gap and filled up effect.
4. the present invention can evaporate solvent successively by the way of gradient vacuum distillation, prevent evaporation of the solvent too fast, cause
Particle aggregation.
5. polyvinylpyrrolidone is sintered removal by the present invention by the way of sintering, and using polymethyl
Sour methyl esters is filled up agent as gap and can effectively be filled up gap, at the same can also be formed under the conditions of gradient sintering it is hard and soft simultaneously
The bullet proof composite plating of Ji.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
The described technical solution of inventive embodiments.It will be understood by those of ordinary skill in the art that still the present invention can be carried out
Modification or equivalent replacement, to reach identical technique effect；As long as meeting using needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of high-performance bullet proof composite plating, it is characterised in that：The preparation method is in accordance with the following steps：
Step 1, aluminum soluble salt is added in deionized water, is then slowly added into ammonium hydroxide, until precipitation no longer generates, stand 1-
3h obtains aluminium hydroxide suspension；
Step 2, it adds a dispersant in aluminium hydroxide suspension, ultrasonic reaction 10-30min obtains suspended dispersion liquid；
Step 3, graphene particles are added in absolute ethyl alcohol, then mechanical agitation seals ultrasonic reaction to dispersion effect is formed
20-30min obtains activated graphene suspension；
Step 4, activated graphene suspension is slowly added into suspended dispersion liquid, is uniformly mixing to obtain mixed liquor；
Step 5, mixed liquor is added in into reaction kettle and forms gradient vacuum distillation reaction 5-8h, obtain viscous fluid；
Step 6, viscous fluid is put into mold and is sintered 10-15h, added in polymethyl methacrylate solution and surpass after natural cooling
Phonoresponse 2-5h, flash baking after taking-up obtain the prefabricated armour of plated film；
Step 7, the prefabricated armour of plated film is added in into gradient sintering 10-12h in reaction kettle, high-performance bulletproof composite is obtained after cooling
Plate.
2. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 1
Aluminum soluble salt using aluminium chloride, the mass concentration of the aluminum soluble salt in deionized water is 10-30g/L.
3. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 1
In ammonia add in speed be 10-30mL/min, the dwell temperature be 60-70 DEG C.
4. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 2
In dispersant using polyvinylpyrrolidone, the addition of the dispersant is the 20-40% of aluminium salt quality, and the ultrasound is anti-
The frequency answered is 2.5-7.5kHz, and temperature is 70-80 DEG C.
5. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 3
In graphene particles grain size no more than 100 μm, a concentration of 10-30g/L in absolute ethyl alcohol, the graphene particles
Addition is the 40-60% of aluminium salt, and the churned mechanically speed is 2000-4000r/min, and the sealing ultrasonic reaction uses
Water bath sonicator reacts, supersonic frequency 5.5-10.5kHz, and temperature is 60-70 DEG C.
6. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 4
In activated graphene suspension addition speed for 15-25mL/min, the mixing speed of the stirring is 2000-4000r/
min。
7. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 5
In gradient vacuum distillation reaction using microwave reaction, Gradient program is as follows：
8. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 6
In sintering temperature for 1000-1200 DEG C, the sintering processing is using microwave heating reaction, microwave power 200-400W.
9. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 6
The solvent of middle polymethyl methacrylate solution uses acetone, and the temperature of the ultrasonic reaction is 60-70 DEG C, frequency 10-
30kHz, the drying temperature are 70-90 DEG C.
10. a kind of preparation method of high-performance bullet proof composite plating according to claim 1, it is characterised in that：The step 7
In gradient sintering be sintered using Muffle furnace, Gradient program is as follows：
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| CN108863321A (en) * | 2018-07-10 | 2018-11-23 | 武汉科技大学 | A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof |
| CN109037620A (en) * | 2018-07-12 | 2018-12-18 | 浙江工业职业技术学院 | A kind of silicon based on porous carbon covers the preparation method of composite material |
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| CN108863321A (en) * | 2018-07-10 | 2018-11-23 | 武汉科技大学 | A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof |
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